Characterization of constituents in Stellera chamaejasme L. by rapid-resolution liquid chromatography-diode array detection and electrospray ionization time-of-flight mass spectrometry.

A reliable and rapid method based on rapid-resolution liquid chromatography-diode array detection (RRLC-DAD) and electrospray ionization time-of-flight mass spectrometry (ESI-TOF/MS) has been developed for the isolation and characterization of multiple constituents in the root of Stellera chamaejasme L., which was extracted by sonication with methanol in an optimized procedure. Separation of the multiple constituents was achieved on an Agilent Zorbax XDB-C18 (50x3.0 mm i.d.; 1.8 microm) column using a gradient elution at a flow rate of 0.4 mL/min. The detection wavelength was 210 nm. Mass spectra were acquired in both positive and negative modes. A formula database of the known chemical constituents in the root of Stellera chamaejasme L. was established by an Agilent software. Twenty-two obvious peaks appeared in the total ion chromatogram and nine of them were characterized by TOF/MS. The RRLC-DAD and ESI-TOF/MS method with ultrasonic extraction would be useful for rapid and effective characterization of chemical constituents in the root of Stellera chamaejasme L.

Zhao L ，Lou ZY ，Zhu ZY ，Hai-Zhang ，Zhang GQ ，Chai YF ... -  《BIOMEDICAL CHROMATOGRAPHY》

Rapid separation and identification of phenolic and diterpenoid constituents from Radix Salvia miltiorrhizae by high-performance liquid chromatography diode-array detection, electrospray ionization time-of-flight mass spectrometry and electrospray ionizat

High-performance liquid chromatography-diode array detection (HPLC-DAD), electrospray ionization time-of-flight mass spectrometry (HPLC-ESI-TOF-MS) and electrospray ionization quadrupole ion trap mass spectrometry (HPLC-ESI-MSn) were used for the isolation, identification and structural analysis of water-soluble phenolic and nonpolar diterpenoid constituents in Dan-shen (Radix Salvia miltiorrhizae) which was prepared by sonication in 70% methanol. Mass spectra were obtained by ESI-TOF-MS and electrospray ionization quadrupole ion trap mass spectrometry (ESI-QIT-MS). A formula database of known constituents in Dan-shen was established and most constituents were rapidly identified by HPLC-DAD/ESI-TOF-MS by matching their accurate molecular masses with the formulae of the compounds in the database. Compounds with the same molecular formula could not be differentiated by TOF-MS; however, QIT-MS could differentiate those compounds and elucidate their structures based on their characteristic fragmentation. HPLC-DAD, HPLC/ESI-TOF-MS and HPLC/ESI-MSn provided complementary information for the identification of the constituents in Dan-shen. Forty constituents were identified in 30 min based on their positive and negative ion ESI mass spectra and liquid chromatographic information. Thus the method described is useful for the rapid analysis of multiple constituents in Dan-shen.

Zhu Z ，Zhang H ，Zhao L ，Dong X ，Li X ，Chai Y ，Zhang G ... -  《RAPID COMMUNICATIONS IN MASS SPECTROMETRY》

Rapid separation and identification of major constituents in Pseudolarix kaempferi by ultra-performance liquid chromatography coupled with electrospray and quadrupole time-of-flight tandem mass spectrometry.

A rapid and reliable method based on ultra-performance liquid chromatography (UPLC) coupled with photodiode-array detection (PDA) and electrospray ionization quadrupole time-of-flight tandem mass spectrometry (ESI-Q-TOF-MS/MS) has been developed for separation and identification of major constituents in extracts of root bark of Pseudolarix kaempferi Gordon (PKG). Identification of the constituents was carried out by interpretation of their retention times, UV absorption spectra, MS and MS/MS spectra, as well as the data provided by authentic standards and literatures. A total of 20 components were separated in only 8.0 min on a small particle size C18 column (1.7 microm). These components included nine diterpene acids, seven glycosides and four triterpenoids, among which pseudolaric acid C-O-beta-D-glucopyranoside and pseudolaric acid C2-O-beta-D-glucopyranoside were separated and identified for the first time in this study. Furthermore, the fragmentation patterns of the three types of compounds were elucidated for the first time. This established UPLC-PDA/Q-TOF-MS/MS method is reliable and effective for the separation and identification of the 20 compounds and will be useful for quality control of the crude materials of Pseudolarix kaempferi Gordon and their related preparations.

Ye X ，Tang M ，Chen L ，Peng A ，Ma L ，Ye H ... -  《-》

Simultaneous analysis of coumarins and secoiridoids in Cortex Fraxini by high-performance liquid chromatography-diode array detection-electrospray ionization tandem mass spectrometry.

Zhou L ，Kang J ，Fan L ，Ma XC ，Zhao HY ，Han J ，Wang BR ，Guo DA ... -  《JOURNAL OF PHARMACEUTICAL AND BIOMEDICAL ANALYSIS》

Rapid separation and identification of 54 major constituents in Buyang Huanwu decoction by ultra-fast HPLC system coupled with DAD-TOF/MS.

Buyang Huanwu Decoction (BYHWD), is a well-known traditional Chinese preparation consisting of Radix Astragali, Radix Angelicae Sinensis, Rhizoma Ligustici Chuanxiong, Radix paeoniae Rubra, Flos Carthami, Semen Persicae and Lumbricus. An ultra-fast high-performance liquid chromatography (HPLC) method coupled with diode array detection (DAD) and electrospray ionization time-of-flight mass spectrometry (ESI-TOF/MS) has been developed for rapid separation and structural identification of constituents in BYHWD. Using an ultra-fast HPLC system with short columns (4.6 x 50 mm, 1.8 microm), the total analysis time for this complex prescription is less than 30 min. With various fragmentor voltages in TOF/MS, accurate mass measurements (less than 5 ppm error) for molecular ions and characteristic fragment ions could represent reliable identification criteria for these compounds. Fifty-four major constituents from BYHWD sample, including four C-glycosyl quinochalcones, four flavonoid O-glycosides, sixteen isoflavones, six monoterpene glycosides, eight saponins, four organic acids and five amino acids, were identified or tentatively characterized based on their retention times, DAD and TOF/MS data. All the compounds were further assigned in the seven individual crude drugs. In conclusion, the ultra-fast HPLC with DAD-TOF/MS is a highly useful and efficient technique to separate and identify constituents in complex matrices of herbal medicines or preparations.

Liu EH ，Qi LW ，Peng YB ，Cheng XL ，Wu Q ，Li P ，Li CY ... -  《-》